CN113699424A - High-entropy alloy material, surface laser remelting method and gradient high-entropy alloy material - Google Patents
High-entropy alloy material, surface laser remelting method and gradient high-entropy alloy material Download PDFInfo
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Abstract
Disclosed herein are a high-entropy alloy material, a surface laser remelting method, and a gradient high-entropy alloy material. Wherein the high-entropy alloy material is CoCrFeMnNi alloy, and the shape of the high-entropy alloy material is a single-phase face-centered cubic structure; the high-entropy alloy comprises the following components in atomic percentage: 5 to 35at percent of Co, 5 to 35at percent of Cr, 5 to 35at percent of Fe, 5 to 35at percent of Mn, 5 to 35at percent of Ni, and the sum of the atomic percentages of the components is 100at percent. The surface of the CoCrFeMnNi high-entropy alloy material is subjected to laser remelting treatment, the laser output power is 500W-2500W, and the gradient high-entropy alloy material with the grain size gradually increasing from the surface to the center is obtained, so that the surface hardness, the surface wear resistance and the compressive strength of the CoCrFeMnNi high-entropy alloy are greatly improved.
Description
Technical Field
The invention relates to the technical field of laser processing, in particular to a high-entropy alloy material, a surface laser remelting method and a gradient high-entropy alloy material.
Background
Taiwan scholars Yun Yu in 2004 proposed the design concept of high entropy alloy, which is a multi-component alloy composed of 5 or more than 5 elements in equal or nearly equal molar ratio, and the mole fraction of each element is between 5% and 35%. In 2004, the teaching of Cantor reports for the first time that a high-entropy alloy of a single-phase face-centered cubic structure, namely, cocrfmni, has excellent low-temperature mechanical properties, but the strength of the alloy at room temperature is very low, so that the application of the alloy is limited to a certain extent, and therefore, a technology is urgently needed to greatly improve the strength of the cocrfmni high-entropy alloy.
The laser remelting technology is to melt the surface of a material by using a high-energy laser beam without adding any metal element, thereby achieving the purpose of improving the surface structure. The laser remelting technology can refine the structure and eliminate pores and cracks on the surface of the alloy.
The CoCrFeMnNi high-entropy alloy has low strength and is limited in application in practical life, and in order to obtain excellent structure performance and perfect the research of laser surface treatment on the microstructure, mechanical property and corrosion property of the high-entropy alloy, the CoCrFeMnNi high-entropy alloy is subjected to surface remelting by using different laser powers to improve the comprehensive performance of the CoCrFeMnNi high-entropy alloy.
In view of this, the invention is particularly proposed.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a high-entropy alloy material, a surface laser remelting method and a gradient high-entropy alloy material.
The invention is realized by the following steps:
the invention provides a high-entropy alloy material, wherein the high-entropy alloy is a CoCrFeMnNi alloy, the appearance of the high-entropy alloy is a single-phase face-centered cubic structure, and the high-entropy alloy comprises the following components in atomic percentage: 5 to 35at percent of Co, 5 to 35at percent of Cr, 5 to 35at percent of Fe, 5 to 35at percent of Mn, 5 to 35at percent of Ni, and the sum of the atomic percentages of the components is 100at percent.
The invention also provides a preparation method of the high-entropy alloy material, which comprises the following steps: high-purity materials are selected and accurately weighed and proportioned according to an equimolar ratio, and then are smelted and annealed under a vacuum condition to obtain the high-entropy alloy material.
The invention also provides a surface laser remelting method of the high-entropy alloy material, which comprises the following steps: and performing laser irradiation on the surface of the high-entropy alloy material by using a laser to form a laser remelting layer.
The invention also provides a gradient high-entropy alloy material prepared by the preparation method.
The invention has the following beneficial effects:
the invention provides a high-entropy alloy material, a surface laser remelting method and a gradient high-entropy alloy material, wherein the high-entropy alloy is a CoCrFeMnNi alloy, and the shape of the high-entropy alloy is a single-phase face-centered cubic structure; the high-entropy alloy comprises the following components in atomic percentage: 5 to 35at percent of Co, 5 to 35at percent of Cr, 5 to 35at percent of Fe, 5 to 35at percent of Mn, 5 to 35at percent of Ni, and the sum of the atomic percentages of the components is 100at percent. The surface of the CoCrFeMnNi high-entropy alloy material is subjected to laser remelting treatment, the laser output power is 500W-2500W, the gradient high-entropy alloy material with the grain size gradually changing from the surface to the center is obtained, the surface hardness of the cast CoCrFeMnNi high-entropy alloy is improved from 156HV to 174-3200 HV, the compressive strength is improved from 2450MPa to 2480-3200MPa, the average friction coefficient of the surface of the cast CoCrFeMnNi high-entropy alloy is changed from 0.124 to 0.099-0.127, and the wear resistance is further improved.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.
FIG. 1 is an XRD diffraction pattern of a CoCrFeMnNi high-entropy alloy in an as-cast state and subjected to laser remelting treatment under different laser powers.
FIG. 2 is a Zeiss microscope picture of as-cast CoCrFeMnNi high-entropy alloy and after laser remelting treatment under different laser powers, wherein: (a) as-cast, (b)500W, (c)1000W, (d)1500W, (e)2000W, (f) 2500W.
FIG. 3 is a distribution diagram of isometric crystal grain size from the surface to the core of an as-cast CoCrFeMnNi high-entropy alloy after laser remelting treatment under different laser powers, wherein: (a)500W, (b)1000W, (c)1500W, (d)2000W, (e) 2500W.
FIG. 4 is a topographical image of the surface and cross-section of a sample after 3000W laser remelting treatment, wherein: (a) surface, (b) cross-section.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
The invention aims to develop a high-entropy alloy material, a surface laser remelting method and a gradient high-entropy alloy material, and particularly provides a CoCrFeMnNi high-entropy alloy surface strengthened by adopting different laser remelting powers. Therefore, the high-entropy alloy has higher strength and good plasticity.
In order to achieve the purpose, the technical scheme adopted by the invention for achieving the purpose is as follows:
in a first aspect, embodiments of the present invention provide a high-entropy alloy material, where the high-entropy alloy is a cocrfmnni alloy, and the shape of the alloy is a single-phase face-centered cubic structure; the high-entropy alloy comprises the following components in atomic percentage: 5 to 35at percent of Co, 5 to 35at percent of Cr, 5 to 35at percent of Fe, 5 to 35at percent of Mn, 5 to 35at percent of Ni, and the sum of the atomic percentages of the components is 100at percent.
Further preferably, an embodiment of the present invention provides a quinary-equivalent high entropy alloy material, which is composed of, in atomic percentage, 20 at% of Co, 20 at% of Cr, 20 at% of Fe, 20 at% of Mn, and 20 at% of Ni.
In a second aspect, an embodiment of the present invention provides a preparation method of the above high-entropy alloy material, including the following steps:
(1) preparing materials: respectively weighing simple substance raw materials of Co, Cr, Fe, Mn and Ni according to mass percentage;
(2) smelting: A. putting the simple substance raw materials Co, Cr, Fe, Mn and Ni weighed in the step (1) into a water-cooled copper crucible in a vacuum suspension smelting furnace; B. closing the furnace door of the vacuum suspension smelting furnace, and screwing down the knob; C. vacuumizing the vacuum suspension smelting furnace to make the vacuum degree reach 5 x 10-5-5×10-3Pa; d. Repeatedly smelting the alloy for 5-8 times, and carrying out vacuum casting in stainless steel casting equipment to obtain the quinary high-entropy alloy cast ingot.
(3) Annealing treatment: annealing the five-element high-entropy alloy cast ingot at the temperature of 1100-1300 ℃, preserving the heat for 12-36h, taking out the five-element high-entropy alloy cast ingot, and performing water quenching to obtain a homogenized high-entropy alloy sample.
Furthermore, the purity of Co, Cr, Fe, Mn and Ni is equal to or larger than 99%.
Further, Co, Cr, Fe, Mn, and Ni are in the form of blocks.
Further, vacuum degree is pumped to 5X 10 during smelting-5Pa; repeatedly smelting the alloy for 6 times, carrying out vacuum casting in stainless steel casting equipment to prepare a quinary high-entropy alloy ingot, then carrying out annealing treatment at 1200 ℃, keeping the temperature for 24 hours, taking out, and then taking out for water quenching to obtain a homogenized high-entropy alloy sample.
In a third aspect, an embodiment of the present invention further provides a surface laser remelting method for the ladder high-entropy alloy material, including the following steps:
(1) and removing oxide skin on the surface of the CoCrFeMnNi high-entropy alloy sample subjected to annealing treatment by using SiC sand paper.
(2) And soaking the polished CoCrFeMnNi high-entropy alloy sample in absolute ethyl alcohol, and putting the sample into an ultrasonic cleaner for vibration cleaning to remove surface oil stains.
(3) Laser remelting treatment: the surface was subjected to laser remelting treatment using a TruDisk 6002 laser, with laser treatment powers of 500W, 1000W, 1500W, 2000W, 2500W, and 3000W, respectively, a laser spot diameter d of 4mm, and a scanning speed v of 20 mm/s. Argon gas is used as shielding gas, and the flow of the shielding gas is 15 L.min-1。
In a fourth aspect, the embodiment of the invention also provides a gradient high-entropy alloy material prepared by the preparation method.
Preferably, the thickness of the laser remelting layer is 0.2mm-2.4mm, and the surface of the remelting layer is free of defects and cracks.
Preferably, the gradient high-entropy alloy is a CoCrFeMnNi alloy, the appearance of the alloy is a single-phase face-centered cubic structure, the grain size of the alloy gradually increases from the surface to the center, and the atomic percentages of the components of the gradient high-entropy alloy are as follows: 5 to 35at percent of Co, 5 to 35at percent of Cr, 5 to 35at percent of Fe, 5 to 35at percent of Mn, 5 to 35at percent of Ni, and the sum of the atomic percentages of the components is 100at percent.
Compared with the prior art, the invention has the advantages and beneficial effects that:
(1) in the laser remelting process, the laser can melt and re-solidify the surface layer of the CoCrFeMnNi high-entropy alloy, and defects such as air holes, cracks and the like existing in the surface layer of the CoCrFeMnNi high-entropy alloy can be eliminated in the process.
(2) The laser remelting layer obtained by laser remelting has high hardness, and has good wear resistance and compressive strength.
The features and properties of the present invention are described in further detail below with reference to examples.
In the following examples of the present invention, the raw material sources, components, preparation and experimental methods were the same as those of the comparative examples.
Example 1
The preparation method of the CoCrFeMnNi high-entropy alloy subjected to laser remelting treatment in the as-cast state and under different laser powers comprises the following specific steps:
(1) preparing materials: the high-purity massive metal raw material (more than or equal to 99 percent) is accurately weighed and proportioned according to mass percent for smelting alloy.
(2) Smelting: A. putting the simple substance raw materials Co, Cr, Fe, Mn and Ni weighed in the step (1) into a water-cooled copper crucible in a vacuum suspension smelting furnace; B. closing the furnace door of the vacuum suspension smelting furnace, and screwing down the knob; C. vacuumizing the vacuum suspension smelting furnace to make the vacuum degree reach 5 x 10-5Pa; D. repeatedly smelting the alloy for 6 times, and carrying out vacuum casting in stainless steel casting equipment to prepare the quinary high-entropy alloy cast ingot.
(3) Annealing treatment: and annealing the alloy ingot at 1200 ℃, keeping the temperature for 24h, and taking out for water quenching.
(4) And removing oxide skin on the surface of the annealed CoCrFeMnNi high-entropy alloy by using SiC sand paper.
(5) And soaking the polished CoCrFeMnNi high-entropy alloy in absolute ethyl alcohol, and putting the soaked CoCrFeMnNi high-entropy alloy into an ultrasonic cleaner for vibration cleaning to remove surface oil stains.
(6) Laser remelting treatment: and performing laser remelting treatment on the surface of the ingot by using a TruDisk 6002 laser, wherein the laser treatment power is 500W, the laser spot diameter d is 4mm, and the scanning speed v is 20 mm/s.
(7) Argon gas is used as shielding gas, and the flow of the shielding gas is 15 L.min-1。
The structural characterization and mechanical property test of the 500W laser remelting CoCrFeMnNi prepared in this example showed the following results:
(1) x-ray diffraction (XRD) testing and phase composition analysis
Cutting a required sample from the block sample subjected to the remelting treatment on the laser surface by using a wire cutting machine, gradually grinding the sample by using sand paper of 400#, 800#, 1000#, 1500#, 2000#, washing the sample by using alcohol after polishing, and drying the sample by blowing, thereby obtaining a smooth and flat plane for XRD analysis, wherein the scanning angle 2 theta range is 20-90 degrees, and the scanning speed is 40 degrees/min.
(2) Zeiss microscope tissue observation and analysis
Cutting the block sample subjected to the laser surface remelting treatment into a sample required by a test by using a wire cutting machine, inlaying the section and the surface of the remelted layer by using bakelite powder, and gradually polishing by using sand paper of No. 400, No. 800, No. 1000, No. 1500, No. 2000. And (3) washing the polished sample with alcohol, corroding the surface of the sample with aqua regia, and observing the structure of the corroded sample by using a Zeiss microscope.
(3) Alloy compression test
A linear cutting machine is adopted to process a sample into a cylindrical sample, the upper surface and the lower surface of the cylinder are surfaces subjected to laser remelting, the size of the cylindrical sample is 5mm in diameter and 10mm in height, and the surface of the sample before compression is polished to be horizontal by abrasive paper. If the two ends are not horizontal, errors will be generated in the compression process, and the test result is influenced. The sample is compressed by a KRYAW-300C pressure tester at room temperature, so that the height of the sample is deformed by 90%, and a stress-strain curve of the sample is obtained by software of the instrument.
(4) Hardness test of alloy
Cutting the alloy wire into round rods with certain lengths, then inlaying the round rods, after inlaying, roughly grinding the round rods by using 100# abrasive paper, and then grinding and polishing the surfaces of the samples by using silicon carbide abrasive paper with different grain sizes (according to the sequence of 400#, 800#, 1000#, and 1500 #). The alloy hardness is measured by using a Vickers microhardness tester, the selected load in the experiment is 3N, the load holding time is 15s, and the hardness value is read after unloading. 10 sets of hardness values were measured and recorded for each sample and the average was calculated.
(5) Frictional wear performance test
The sample was processed into a block-shaped test piece having a size of 10mm × 10mm × 5mm using a wire cutter, and the surface of the test piece was ground and polished with silicon carbide sandpaper (400 #, 800#, 1000#, 1500 #) having different particle sizes. The friction and wear test is carried out by adopting an MFT-4000 type multifunctional material surface performance tester, the constant-load reciprocating friction is carried out on the surface of a sample, the loading load is 15N, the speed is 100mm/min, the length of a grinding mark is 5mm, and then the abrasion loss analysis is carried out on the sample.
The average friction coefficient of the surface of the CoCrFeMnNi high-entropy alloy after the 500W laser remelting treatment is 0.124, and the abrasion loss of a corresponding high-entropy alloy treatment layer is 0.00328mm3。
Example 2
The preparation method of the CoCrFeMnNi high-entropy alloy subjected to laser remelting treatment in the cast state and under different laser powers comprises the following specific steps:
(1) preparing materials: the high-purity massive metal raw material (more than or equal to 99 percent) is accurately weighed and proportioned according to mass percent for smelting alloy.
(2) Smelting: A. putting the simple substance raw materials Co, Cr, Fe, Mn and Ni weighed in the step (1) into a water-cooled copper crucible in a vacuum suspension smelting furnace; B. closing the furnace door of the vacuum suspension smelting furnace, and screwing down the knob; C. vacuumizing the vacuum suspension smelting furnace to make the vacuum degree reach 5 x 10-5Pa; D. repeatedly smelting the alloy for 6 times, and carrying out vacuum casting in stainless steel casting equipment to prepare the quinary high-entropy alloy cast ingot.
(3) Annealing treatment: and annealing the alloy ingot at 1200 ℃, keeping the temperature for 24h, and taking out for water quenching.
(4) And removing oxide skin on the surface of the annealed CoCrFeMnNi high-entropy alloy by using SiC sand paper.
(5) And soaking the polished CoCrFeMnNi high-entropy alloy in absolute ethyl alcohol, and putting the soaked CoCrFeMnNi high-entropy alloy into an ultrasonic cleaner for vibration cleaning to remove surface oil stains.
(6) Laser remelting treatment: and performing laser remelting treatment on the surface of the ingot by using a TruDisk 6002 laser, wherein the laser treatment power is 1000W, the laser spot diameter d is 4mm, and the scanning speed v is 20 mm/s.
(7) Argon gas is used as shielding gas, and the flow of the shielding gas is 15 L.min-1。
The 1000W laser remelting treatment cocrfermni prepared in this example was subjected to structural characterization and mechanical property testing, and the results were as follows:
(1) x-ray diffraction (XRD) testing and phase composition analysis
Cutting a required sample from the block sample subjected to the remelting treatment on the laser surface by using a wire cutting machine, gradually grinding the sample by using sand paper of 400#, 800#, 1000#, 1500#, 2000#, washing the sample by using alcohol after polishing, and drying the sample by blowing, thereby obtaining a smooth and flat plane for XRD analysis, wherein the scanning angle 2 theta range is 20-90 degrees, and the scanning speed is 40 degrees/min.
(2) Zeiss microscope tissue observation and analysis
Cutting the block sample subjected to the laser surface remelting treatment into a sample required by a test by using a wire cutting machine, inlaying the section and the surface of the remelted layer by using bakelite powder, and gradually polishing by using sand paper of No. 400, No. 800, No. 1000, No. 1500, No. 2000. And (3) washing the polished sample with alcohol, corroding the surface of the sample with aqua regia, and observing the structure of the corroded sample by using a Zeiss microscope.
(3) Alloy compression test
A linear cutting machine is adopted to process a sample into a cylindrical sample, the upper surface and the lower surface of the cylinder are surfaces subjected to laser remelting, the size of the cylindrical sample is 5mm in diameter and 10mm in height, and the surface of the sample before compression is polished to be horizontal by abrasive paper. If the two ends are not horizontal, errors will be generated in the compression process, and the test result is influenced. The sample is compressed by a KRYAW-300C pressure tester at room temperature, so that the height of the sample is deformed by 90%, and a stress-strain curve of the sample is obtained by software of the instrument.
(4) Hardness test of alloy
Cutting the alloy wire into round rods with certain lengths, then inlaying the round rods, after inlaying, roughly grinding the round rods by using 100# abrasive paper, and then grinding and polishing the surfaces of the samples by using silicon carbide abrasive paper with different grain sizes (according to the sequence of 400#, 800#, 1000#, and 1500 #). The alloy hardness is measured by using a Vickers microhardness tester, the selected load in the experiment is 3N, the load holding time is 15s, and the hardness value is read after unloading. 10 sets of hardness values were measured and recorded for each sample and the average was calculated.
(5) Frictional wear performance test
The sample was processed into a block-shaped test piece having a size of 10mm × 10mm × 5mm using a wire cutter, and the surface of the test piece was ground and polished with silicon carbide sandpaper (400 #, 800#, 1000#, 1500 #) having different particle sizes. The friction and wear test is carried out by adopting an MFT-4000 type multifunctional material surface performance tester, the constant-load reciprocating friction is carried out on the surface of a sample, the loading load is 15N, the speed is 100mm/min, the length of a grinding mark is 5mm, and then the abrasion loss analysis is carried out on the sample.
1000W laser remeltingThe average friction coefficient of the surface of the treated CoCrFeMnNi high-entropy alloy is the minimum of 0.099, and the abrasion loss of a corresponding high-entropy alloy treatment layer is the minimum of 0.00127mm3. This shows that the CoCrFeMnNi high-entropy alloy surface after 1000W laser remelting has the best frictional wear performance.
Example 3
The preparation method of the as-cast and 1500W laser remelting CoCrFeMnNi high-entropy alloy comprises the following specific steps:
(1) preparing materials: the high-purity massive metal raw material (more than or equal to 99 percent) is accurately weighed and proportioned according to mass percent for smelting alloy.
(2) Smelting: A. putting the simple substance raw materials Co, Cr, Fe, Mn and Ni weighed in the step (1) into a water-cooled copper crucible in a vacuum suspension smelting furnace; B. closing the furnace door of the vacuum suspension smelting furnace, and screwing down the knob; C. vacuumizing the vacuum suspension smelting furnace to make the vacuum degree reach 5 x 10-5Pa; D. repeatedly smelting the alloy for 6 times, and carrying out vacuum casting in stainless steel casting equipment to prepare the quinary high-entropy alloy cast ingot.
(3) Annealing treatment: and annealing the alloy ingot at 1200 ℃, keeping the temperature for 24h, and taking out for water quenching.
(4) And removing oxide skin on the surface of the annealed CoCrFeMnNi high-entropy alloy by using SiC sand paper.
(5) And soaking the polished CoCrFeMnNi high-entropy alloy in absolute ethyl alcohol, and putting the soaked CoCrFeMnNi high-entropy alloy into an ultrasonic cleaner for vibration cleaning to remove surface oil stains.
(6) Laser remelting treatment: and performing laser remelting treatment on the surface of the ingot by using a TruDisk 6002 laser, wherein the laser treatment power is 1500W, the laser spot diameter d is 4mm, and the scanning speed v is 20 mm/s.
(7) Argon gas is used as shielding gas, and the flow of the shielding gas is 15 L.min-1。
The 1500W laser remelting treatment CoCrFeMnNi prepared by the embodiment is subjected to organizational structure characterization and mechanical property test, and the results are as follows:
(1) x-ray diffraction (XRD) testing and phase composition analysis
Cutting a required sample from the block sample subjected to the remelting treatment on the laser surface by using a wire cutting machine, gradually grinding the sample by using sand paper of 400#, 800#, 1000#, 1500#, 2000#, washing the sample by using alcohol after polishing, and drying the sample by blowing, thereby obtaining a smooth and flat plane for XRD analysis, wherein the scanning angle 2 theta range is 20-90 degrees, and the scanning speed is 40 degrees/min.
(2) Zeiss microscope tissue observation and analysis
Cutting the block sample subjected to the laser surface remelting treatment into a sample required by a test by using a wire cutting machine, inlaying the section and the surface of the remelted layer by using bakelite powder, and gradually polishing by using sand paper of No. 400, No. 800, No. 1000, No. 1500, No. 2000. And (3) washing the polished sample with alcohol, corroding the surface of the sample with aqua regia, and observing the structure of the corroded sample by using a Zeiss microscope.
(3) Alloy compression test
A linear cutting machine is adopted to process a sample into a cylindrical sample, the upper surface and the lower surface of the cylinder are surfaces subjected to laser remelting, the size of the cylindrical sample is 5mm in diameter and 10mm in height, and the surface of the sample before compression is polished to be horizontal by abrasive paper. If the two ends are not horizontal, errors will be generated in the compression process, and the test result is influenced. The sample is compressed by a KRYAW-300C pressure tester at room temperature, so that the height of the sample is deformed by 90%, and a stress-strain curve of the sample is obtained by software of the instrument.
(4) Hardness test of alloy
Cutting the alloy wire into round rods with certain lengths, then inlaying the round rods, after inlaying, roughly grinding the round rods by using 100# abrasive paper, and then grinding and polishing the surfaces of the samples by using silicon carbide abrasive paper with different grain sizes (according to the sequence of 400#, 800#, 1000#, and 1500 #). The alloy hardness is measured by using a Vickers microhardness tester, the selected load in the experiment is 3N, the load holding time is 15s, and the hardness value is read after unloading. 10 sets of hardness values were measured and recorded for each sample and the average was calculated.
(5) Frictional wear performance test
The sample was processed into a block-shaped test piece having a size of 10mm × 10mm × 5mm using a wire cutter, and the surface of the test piece was ground and polished with silicon carbide sandpaper (400 #, 800#, 1000#, 1500 #) having different particle sizes. The friction and wear test is carried out by adopting an MFT-4000 type multifunctional material surface performance tester, the constant-load reciprocating friction is carried out on the surface of a sample, the loading load is 15N, the speed is 100mm/min, the length of a grinding mark is 5mm, and then the abrasion loss analysis is carried out on the sample.
The average friction coefficient of the surface of the CoCrFeMnNi high-entropy alloy after the 1500W laser remelting treatment is 0.115, and the abrasion loss of a corresponding high-entropy alloy treatment layer is 0.0083mm3。
FIG. 1 shows XRD diffraction patterns of the as-cast CoCrFeMnNi high-entropy alloy and the laser remelting treatment under different laser powers, and as can be seen from FIG. 1, the solid solution phases of the high-entropy alloy remelted under five different laser powers and the untreated as-cast high-entropy alloy are simple and are single FCC phases, and each phase consists of three diffraction peaks (111), (200) and (220). The phase (111) which is the highest peak among these appears at 2 θ ≈ 43 °, while the (200) and (220) FCC phases appear at 2 θ ≈ 51 ° and 2 θ ≈ 75 °. With the increase of the laser power, no new diffraction peak appears, namely, the change of the laser power does not cause the alloy to generate a new phase, so that the gradient high-entropy alloy is known to have good thermal stability.
FIG. 2 is a Zeiss microscope picture of as-cast CoCrFeMnNi high-entropy alloy and after laser remelting treatment under different laser powers. As can be seen from the graph a in FIG. 2, the crystal grains of the as-cast CoCrFeMnNi high-entropy alloy are coarse isometric grains, and the as-cast CoCrFeMnNi high-entropy alloy is observed to have more casting defects under a microscope, and the size of the crystal grains is about 200 μm. After remelting the alloy with a laser at 500W, a remelted layer having a thickness of about 240 μm was formed on one surface of the alloy, as shown in b of FIG. 2. The thickness of the surface remelting region gradually increases with the increase of the laser power, and the thickness of the surface remelting layer is 790 μm, 1300 μm, 1500 μm and 2400 μm when the laser remelting power is 1000W, 1500W, 2000W and 2500W. After laser melting, the remelted layer is rapidly solidified, and the grain size is obviously refined. However, as the laser power increases, the thickness of the remelted layer increases, and the volume fraction of dendrites in the remelted layer gradually increases. The grain size variation is shown in figure 3.
FIG. 3 is a distribution diagram of isometric crystal grain size from the surface to the center of an as-cast CoCrFeMnNi high-entropy alloy after laser remelting treatment under different laser powers. After the 500W laser surface remelting treatment, the equiaxed grain size of the remelted layer was 6 μm, the equiaxed grain size of the heat affected zone was 10 μm, and the equiaxed grain size of the central substrate zone was 253 μm (fig. 3, a). After the 1000W laser surface remelting treatment, the equiaxed grain size of the remelted layer was 5.5 μm, the equiaxed grain size of the heat affected zone was 7.5 μm, and the equiaxed grain size of the central substrate zone was 255um (fig. 3 b). After the 1500W laser surface remelting treatment, the equiaxed grain size of the remelted layer was 4 μm, the equiaxed grain size of the heat affected zone was 7.5 μm, and the equiaxed grain size of the central substrate zone was 245 μm (fig. 3, c). After the 2000W laser surface remelting treatment, the remelted layer had an equiaxed grain size of 3 μm, the heat affected zone had an equiaxed grain size of 6 μm, and the central substrate zone had an equiaxed grain size of 250 μm (fig. 3, d). After the 2500W laser surface remelting treatment, the remelted layer had an equiaxed grain size of 2 μm, the heat affected zone had an equiaxed grain size of 5.3 μm, and the central substrate zone had an equiaxed grain size of 268 μm (fig. 3, panel e).
FIG. 4 is a topographical view of the surface and cross-section of a sample after 3000W laser remelting. As can be seen from FIG. 4, when the laser power was 3000W, the sample was remelted over a large area due to too high output power, and the remelted layer had a thickness of 3.5mm, resulting in excessive surface roughness of the sample (graph a in FIG. 4) and occurrence of bending deformation (graph b in FIG. 4). Therefore, the 500-2500W of the invention has the best effect within the limit of the invention.
The following table 1 shows the mechanical property results of the as-cast alloy and the alloys with different laser remelting powers.
TABLE 1 mechanical Property results for as-cast and different laser remelting Power alloys
As can be seen from Table 1, after the surface melting treatment by laser, the surface hardness of the as-cast CoCrFeMnNi high-entropy alloy is increased from 156.7HV to 174.3-204.1HV, the surface hardness is increased along with the increase of the laser power, and the surface hardness of the high-entropy alloy is the maximum at 2500W. In the compression test, no fracture occurred in each sample, indicating that the pattern had good plasticity. The compressive strength of the as-cast CoCrFeMnNi high-entropy alloy is improved from 2450MPa to 2480-3200MPa, which is caused by the fact that the compressive strength is improved as the thickness of the hard remelted layer is increased along with the increase of the laser power. When the laser power is 500W, the thickness of the hard remelted layer is only 0.2mm, the improvement effect on the compressive strength is very limited, when the laser power is 2500W, the thickness of the hard remelted layer is 2.4mm, the compressive strength is as high as 3200MPa, and the compressive strength is improved by 30.6 percent relative to that of the cast CoCrFeMnNi high-entropy alloy. The average friction coefficient of the surface of the as-cast CoCrFeMnNi high-entropy alloy is changed from 0.124 to 0.099-0.127, and when the laser power is 1000W, the average friction coefficient and the abrasion loss of the surface of the remelting layer are minimum, and the abrasion resistance is best. When the laser power is 3000W, the output power is too high, the sample is remelted in a large area, and the sample is deformed. Obvious defects exist in the remelted layer, the surface roughness is large, and the wear resistance of the sample is reduced.
In summary, the embodiment of the invention provides a high-entropy alloy material, a surface laser remelting method and a gradient high-entropy alloy material, wherein the high-entropy alloy is a CoCrFeMnNi alloy, and the shape of the high-entropy alloy is a single-phase face-centered cubic structure; the high-entropy alloy comprises the following components in atomic percentage: 5 to 35at percent of Co, 5 to 35at percent of Cr, 5 to 35at percent of Fe, 5 to 35at percent of Mn, 5 to 35at percent of Ni, and the sum of the atomic percentages of the components is 100at percent. The surface of the CoCrFeMnNi high-entropy alloy material is subjected to laser remelting treatment, the laser output power is 500W-2500W, and the gradient high-entropy alloy material with the grain size gradually changing from the surface to the center is obtained, so that the surface hardness, the surface wear resistance and the compressive strength of the CoCrFeMnNi high-entropy alloy are greatly improved.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The high-entropy alloy material is characterized in that the high-entropy alloy is a CoCrFeMnNi alloy, the appearance of the high-entropy alloy is a single-phase face-centered cubic structure, and the high-entropy alloy comprises the following components in atomic percentage: 5 to 35at percent of Co, 5 to 35at percent of Cr, 5 to 35at percent of Fe, 5 to 35at percent of Mn, 5 to 35at percent of Ni, and the sum of the atomic percentages of the components is 100at percent.
2. A high entropy alloy material according to claim 1, characterized in that it is a high entropy alloy material of quinary or the like, consisting of, in atomic percentage, 20 at% of Co, 20 at% of Cr, 20 at% of Fe, 20 at% of Mn, and 20 at% of Ni.
3. A method for producing a high-entropy alloy material according to claim 1 or 2, characterized in that it comprises: selecting high-purity materials to be accurately weighed and proportioned according to an equimolar ratio, and then smelting and annealing under a vacuum condition to obtain the high-entropy alloy material.
4. The method of claim 3, comprising the steps of:
smelting: according to the mass percentage, putting the weighed simple substance raw materials of Co, Cr, Fe, Mn and Ni into a water-cooled copper crucible in a vacuum suspension smelting furnace; closing the furnace door of the vacuum suspension smelting furnace, and screwing down the knob; vacuumizing the vacuum suspension smelting furnace to make the vacuum degree reach 5 x 10-5-5×10-3Pa; repeatedly smelting the alloy for 5-8 times, and carrying out vacuum casting in stainless steel casting equipment to prepare a high-entropy alloy cast ingot with the thickness of 10 mm;
annealing: and annealing the obtained high-entropy alloy ingot at the temperature of 1100-1300 ℃, preserving the heat for 12-36h, taking out, and taking out for water quenching to obtain the homogenized high-entropy alloy sample.
5. The preparation method of claim 4, wherein Fe, Co, Ni, Cr and Mn elements selected for smelting are in the form of blocks, the purity of each small simple substance block is not less than 99.99 at%, and vacuum degree is achieved by vacuumizing to 5 x 10 during smelting- 5Pa; repeatedly smelting the alloy for 6 times, and vacuum-casting in stainless steel casting equipmentAnd (3) casting to obtain a gradient high-entropy alloy cast ingot with the thickness of 10mm, then annealing the obtained high-entropy alloy cast ingot at 1200 ℃, keeping the temperature for 24h, taking out the high-entropy alloy cast ingot, and then taking out the high-entropy alloy cast ingot to perform water quenching to obtain a homogenized high-entropy alloy sample.
6. A surface laser remelting method of a high-entropy alloy material is characterized by comprising the following steps: and (3) carrying out laser irradiation on the surface of the high-entropy alloy material by using a laser to form a laser remelted layer, wherein the high-entropy alloy material adopts the high-entropy alloy sample of any one of claims 1-2 or the high-entropy alloy sample prepared by the preparation method of any one of claims 3-5.
7. The surface laser remelting method according to claim 6, comprising the steps of: cleaning the surface of the high-entropy alloy material, and then performing laser irradiation on the surface of the high-entropy alloy material by using a laser to form a laser remelting layer;
preferably, the cleaning process comprises the steps of: firstly, removing oxide skin on the surface of the high-entropy alloy sample subjected to annealing treatment by using SiC sand paper; then soaking the polished high-entropy alloy sample in absolute ethyl alcohol, and putting the sample into an ultrasonic cleaning instrument for vibration cleaning to remove oil stains on the surface;
preferably, the laser irradiation comprises the steps of: adopting TruDisk 6002 laser with output power of 500-3000W, laser spot diameter of 2-4mm, scanning speed of 10-20mm/s, argon as protecting gas and gas flow of 10-15 L.min-1。
8. A gradient high-entropy alloy material produced according to the production method described in any one of claims 6 to 7.
9. A gradient high-entropy alloy material according to claim 8, wherein the thickness of the laser remelted layer is 0.2mm-2.4mm, and the surface of the remelted layer is free of defects and cracks.
10. A gradient high-entropy alloy material according to claim 9, wherein the gradient high-entropy alloy is a cocrfelmni alloy, the morphology of the alloy is a single-phase face-centered cubic structure, the grain size of the alloy gradually increases from the surface to the center, and the atomic percentages of the components of the gradient high-entropy alloy are as follows: 5 to 35at percent of Co, 5 to 35at percent of Cr, 5 to 35at percent of Fe, 5 to 35at percent of Mn, 5 to 35at percent of Ni, and the sum of the atomic percentages of the components is 100at percent.
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